HRID1277814

反应详情

EQUATION

反应方程式

HRID 1277814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

146 mg of phenyl isocyanate was added to a solution of 186 mg (1.2 mmol) of methyl 4-aminopicolate in 4 ml of dry acetone. The resulting mixture was agitated at room temperature overnight. Solvent was then evaporated off and the residue chromatographed in a conventional manner using silica gel (solvent:CHCl3 :acetone=4:1 volume). Fractions were collected and solvent removed by distillation. The residue was recrystallized from methanol to give the desired product having a melting point of 206°-208° C. (decompd.) in an amount of 261 mg (yiled 78.6%).

WORKUP

后处理

  1. customSolvent was then evaporated off
  2. customthe residue chromatographed in a conventional manner
  3. customFractions were collected
  4. customsolvent removed by distillation
  5. customThe residue was recrystallized from methanol